Analytical apparatus



H. B. PULSIFER.

ANALYTICAL APPARATUS.

APPLICATION FILED 050.22, 1919.

Patented May 18, 1920.

Zzfmgisx I UNITED s'rn rns rrrcn HARRIE B. PULSIFER, OF BUTTE, MONTANA, ASS IGNOR TO SCHAAR- & COMPANY, OF CHICAGO, ILLINOIS, A CQR-PQRATION OF ILLINOIS.

ANALYTICAL APPARATUS.

Specification of Letters Patent.

Patented May 18, 1920.

Application filed December 22, 1919. I Serial No. 346,464.

To all whom it may concern Be it known that I, HARRIE B. PULsIrER, a citizen of the United States, residing at Butte, in the county of Silver Bow and State of Montana, have invented certain new and useful Improvements in Analytical Apparatus, of which the following is a specification.

The present invention has to do with certain improvements in analytical apparatus such as used in analytical laboratory work. The apparatus of the present invention is intended particularly for use in the analytical chemistry laboratory and is intended especially for use in determining the sulfur contained in iron and steel by what is known as the evolution method. While the apparatus herein disclosed may be readily used for other purposes than for the determina tion of sulfur in iron and steel, still it is particularly well adapted for this special kind of work. In view of this fact, and in order that the construction and mode of operation of the apparatus may be more readily understood and appreciated by those skilled in the art, I will first explain briefly the evolution method of determining sulfur in iron and steel.

According to this method of determination the sample is cut into relatively small pieces and placed in the beaker or flask which is then closed. Concentrated hydrochloric acid is introducted directly onto the iron or steel particles through a connection, and the sulfur is eliminated through another connection in the form of hydrogen sulfid (H S). The amount of H S is readily determined and from this amount it is easily possible to determine the sulfur inthe original material.

During this process considerable heat is generated and fine particles of acid are thrown up into the upper portion of the beaker. It sometimes happens that fine particles of the iron or steel are in this way carried up and delivered out from the beaker along with the H 8 gas so that the ultimate computation is correspondingly erroneous and inaccurate.

I have discovered the fact that if the upper interior portion of the beaker be cooled as by means of a cooling coil, so that the gases are relatively cooled in the upper portion of the beaker and adjacent to the delivery point from the beaker it is possible effectively to prevent any carrying over of the fine particles of material or acid with the result that the accuracy of the determination is greatly improved. This cooling action serves to condense any acid. which might be carried up into the upper portion of the beaker, such condensed acid dripping back into the bottom of the beaker, and returning with it any fine particles of material.

Bearing the foregoing explanation in mind, reference may be had to the accompanying drawing in which the figure shows a cross section through a beaker having-applied thereto a cooling coil for the above purposes. The beaker is designated by the numeral 1, and may be of any well known or convenient form. In its upper side portion it is provided with a gas delivery connection 2 through which the evolved gases are delivered. The stopper 3 closes the upper end of the beaker. in acid tube t extends vertically down through this stopper from an acid reservoir 5 to a point 6 adjacent to the bottom of the beaker. A pet cock 7 serves as a convenient means for regulating the delivery of acid onto the particles of iron or steel lying in the bottom of the beaker. In conducting the determination the acid is allowed to run down onto the iron and steel particles, its flow being controlled by means of the pet cock.

In the upper portion of the beaker I have provided a cooling coil 8. having its end connections 9 and 10 extending up through the cork or stopper 3. Cooling water or the like may in this manner be readily passed through the coil which will thus cool the gases in the upper portion of the beaker, and before they reach the gas delivery connection 2. It is observed that the end connection 10 of the coil reaches directly to the bottom of the coil at the point 11, so that by introducing the cooling water through the connection 10 the bottom of the coil will be coolest. It is also observed in this connection that by providing a somewhat pointed portion in the lower end of the coil as shown at the point 11 the drippage of the condensate is facilitated and the action of the apparatus correspondingly improved.

Claims:

1. In an analytical apparatus. the combination with a flask havin a throat at its upper end and having a gas delivery connection adjacent to said throat, of a stopper for closing said throat, a vertical acid tube extending through the stopper to a point adj aoent to the bottom of the flask, means for regulating the delivery of acid through said tube, a cooling coil surrounding said tube at a point adjacent to said stopper, and connections from the ends of said coil extending upwardly throu h the stonoer, one of said connections leading directly to the bottom end of the coil and being provided with a relatively pointed lower extremity, substantially as described.

2. In an analytical apparatus, the combination with a flask having a throat in its upper end, and having a gas delivery connection adjacent to said throat, of a closure for the throat, an acid tube extending downwardly through said closure to a point adj acent to the bottom of the flask, and a cooling coil surrounding said acid tube immediately below the closure and having its end portion extending up through the closure to the outside of the apparatus, substantially as described.

3. In an analytical apparatus, the combination with a flask having a throat in its upper end and having a side connection for the delivery of gas, and a closure for said throat, of an acid tube extending through said closure to the interior of the flask, and a cooling coil surrounding said acid tube adjacent to the lower face of the closure, said cooling coil having its end portions extending up through the closure to the outside of the closure, substantially as described.

HARE-IE B. PULSIFER. 

